CN105749946A - Solid alkali catalyst NH4Al(OH)2CO3, method for preparing same and method for catalytically converting glucose by aid of solid alkali catalyst - Google Patents
Solid alkali catalyst NH4Al(OH)2CO3, method for preparing same and method for catalytically converting glucose by aid of solid alkali catalyst Download PDFInfo
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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Abstract
The invention discloses a solid alkali catalyst NH4Al(OH)2CO3, a method for preparing the same and a method for catalytically converting glucose by the aid of the solid alkali catalyst.Aluminum-containing inorganic salt and/or aluminum isopropoxide are used as aluminum sources for the solid alkali catalyst NH4Al(OH)2CO3, urea CO(NH2)2 is used as a precipitating agent for the solid alkali catalyst NH4Al(OH)2CO3, and the solid alkali catalyst can be directly synthesized by the aid of hot liquid without calcinations and activation.The solid alkali catalyst and the methods have the advantages that the method for preparing the solid alkali catalyst is simple, economical and environmentally friendly, and the solid alkali catalyst can be recycled; when the solid alkali catalyst NH4Al(OH)2CO3 is applied to catalytically converting the glucose, the glucose is converted by the aid of the solid alkali catalyst NH4Al(OH)2CO3, ionic liquid 1-butyl-3-methylimidazole chloride and dimethyl sulfoxide to prepare 5-hydroxymethylfurfural, and the ionic liquid 1-butyl-3-methylimidazole chloride and the dimethyl sulfoxide are used as solvents; the solid alkali catalyst is high in yield when used for catalytically converting the glucose to prepare the 5-hydroxymethylfurfural, is easy to separate and low in consumption, can be reused and has an excellent application prospect.
Description
Technical field
The invention belongs to catalyst preparation and applied technical field, be specifically related to a kind of solid base catalyst
NH4Al(OH)2CO3, preparation method and this catalyst prepare the application side in 5 hydroxymethyl furfural in catalysis glucose conversion
Method.
Background technology
Warm along with the worsening shortages of fossil energy, global climate are hurried, environmental pollution constantly aggravates, increasing people
Seek a kind of renewable green energy resource.
In the middle of numerous regenerative resources, biomass energy is the reproducible green energy resource of only one in addition to fossil energy,
The living beings nearly 1.0 × 10 that the whole world is produced by photosynthesis every year11Ton.By biorefinery, biomass energy is permissible
By liquid fuel and high negative value chemicals.As long as and the carbohydrate of biomass derived is living beings parts, the most greatly
Quantifier elimination is devoted to the conversion of biomass derived carbohydrate.
The carbohydrate of biomass derived can obtain a kind of important platform chemicals 5 hydroxymethyl furfural by converting.Pass through
5 hydroxymethyl furfural can prepare various high valuable chemicals further, such as: by rehydration, 5-
Hydroxymethylfurfural can be converted into levulic acid；By selective oxidation, 5 hydroxymethyl furfural can be converted into 2,5-furans
Dimethanol, 2,5-furans dicarbaldehyde and 2,5-furandicarboxylic acid etc..
The catalyst that at present catalysis glucose converts has: tradition is inorganic or organic acid, salt, ionic liquid, solid acid are urged
Agent, solid base catalyst.Although traditional inorganic or organic acid can transforming glucose effectively, but to equipment
Corrosion very serious, increase industrial cost, and be also to have the biggest pollution to environment., the spent acid of generation is the most not
Easily reclaim, can't recycle.Saline catalyst can also prepare 5 hydroxymethyl furfural by transforming glucose, but these
Catalyst is poisonous the most recyclable.Such as CrCl3、AlCl3、ZrCl4Deng.Ionic liquid expensive, it is impossible to real
The large-scale industrial production of row.Comparing some homogeneous catalysts, the advantage of heterogeneous catalysis is clearly.It is nearest
The hot a kind of catalyst of comparison of research, easily separated, recyclable, corrosion-free, nontoxic.But homogeneous catalyst is also
There are disadvantages that, solid catalyst preparation method is complicated, and cost is high, and catalytic efficiency does not has the height of homogeneous catalyst.
In the heterogeneous catalysis of 5 hydroxymethyl furfural is prepared in catalysis glucose conversion, solid acid catalyst account for main group
Becoming part, because numerous studies prove, acid catalyst beneficially glucose is converted into 5 hydroxymethyl furfural.And solid base
It is the most little that 5 hydroxymethyl furfural is prepared in catalyst glucose conversion.With solid base NH4Al(OH)2CO3For catalyst,
5 hydroxymethyl furfural prepared by catalysis glucose, it is not yet reported that mistake.
Summary of the invention
Goal of the invention: in order to overcome the deficiencies in the prior art, the present invention provides a kind of solid base catalyst
NH4Al(OH)2CO3And preparation method thereof, obtain, with simple, economic and environment-friendly, the aluminum carbonate basic ammonium that catalytic efficiency is high.
The present invention also aims to propose the method that 5 hydroxymethyl furfural is prepared in this catalyst efficient catalytic glucose conversion.
Technical scheme: for achieving the above object, the present invention by the following technical solutions:
A kind of solid base catalyst NH4Al(OH)2CO3, this solid base catalyst NH4Al(OH)2CO3Be with containing aluminium without
Machine salt and/or aluminium isopropoxide are aluminium source, urea CO (NH2)2Directly synthesized by hydrothermal solution without calcining and activating for precipitating reagent.
As preferably, described inorganic salt containing aluminium is selected from AlCl3、Al(NO3)3、Al2(SO4)3、AlCl3·6H2O、
Al(NO3)3·9H2O、Al2(SO4)3·16H2One or more in O, wherein AlCl3、AlCl3·6H2O is as containing aluminium
Inorganic salts best results.
Above-mentioned solid base catalyst NH4Al(OH)2CO3Preparation method, comprise the following steps:
(1) using as the inorganic salt containing aluminium in aluminium source and/or aluminium isopropoxide and CO (NH2)2Join in deionized water, so
After constantly agitating solution, until becoming homogeneous phase solution；
(2), after the homogeneous phase solution obtained until step (1) becomes clarification, at once solution is transferred to 100～200mL liners
Reaction in the middle of the reactor of polytetrafluoroethylene (PTFE), then reactor is reacted at 100～300 DEG C 5～60h, when reacted between arrive
When reaching the time of setting, take out reactor, naturally cool to room temperature；
(3) by filtering, wash the reacted product of collection after cooling, at 60～150 DEG C, 3～48h finally it are dried,
I.e. obtain solid base catalyst NH4Al(OH)2CO3。
As preferably, aluminium source and CO (NH in described step (1)2)2The ratio of amount of material be 1-10:1-200.
Invention further provides above-mentioned solid base catalyst NH4Al(OH)2CO3The method of catalyzed conversion glucose,
Said method comprising the steps of:
(1) first by glucose and described solid base catalyst NH4Al(OH)2CO3Join in solvent, obtain mixture
A；
(2) then it is quickly transferred in oil bath stir reaction energetically by the mixture A that step (1) obtains, is reacted
After mixture B；
(3) the mixture B that step (2) obtained adds deionized water and quenches, then with centrifuge with
The speed of 5000～20000rpm separates 3～15min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and product is purple
Outer spectrophotometer is analyzed.
As preferably, in described step (1) reaction dissolvent be 1-butyl-3-methylimidazole villaumite, the one of dimethyl sulfoxide (DMSO)
Planting or the two mixing, wherein 1-butyl-3-methylimidazole villaumite is more excellent with the mixed solution effect of dimethyl sulfoxide (DMSO).
As preferably, in described step (1), solid base catalyst is 3:1 with the mass ratio of glucose.
As preferably, in described step (2), the temperature of oil bath is 60～180 DEG C, and the time of described stirring reaction is 2～12
h。
As preferably, above-mentioned solid base catalyst NH4Al(OH)2CO3The method of catalyzed conversion glucose, concrete steps
As follows
(1) first by 0.01～1g glucose and the solid base catalyst NH of 0.01～5g4Al(OH)2CO3Join 0～10
In the solvent of g1-butyl-3-methylimidazole villaumite and 0～10g dimethyl sulfoxide (DMSO), obtain mixture A, wherein 1-butyl-3-
It is 0 when methylimidazole villaumite is different with dimethyl sulfoxide (DMSO)；
(2) then it is quickly transferred to the mixture A that step (1) obtains in 60～180 DEG C of oil baths stir reaction energetically
2～12h, obtain reacted mixture B；
(3) liquid step (2) obtained adds deionized water to quench, then with centrifuge with 5000～20000rpm
Speed separate 3～15min, collect upper strata hydrolyzate, both 5 hydroxymethyl furfural, product ultraviolet specrophotometer enters
Row is analyzed.
Beneficial effect: compared with prior art, present invention have the advantage that
(1) present invention uses the solid base catalyst NH that hydrothermal method synthesizes4Al(OH)2CO3Preparation method raw material and technique
Extremely simple, cheap, easily separated, can be recycled, environmental protection, there is preferable market application foreground.
(2) this solid base catalyst NH4Al(OH)2CO3When being applied to glucose conversion, product 5 hydroxymethyl furfural
Productivity is higher and catalyst is easily separated, repeatable utilization, expend low.
Accompanying drawing explanation
Fig. 1 is the XRD spectrum of the catalyst aluminum carbonate basic ammonium of embodiment 1 preparation.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is further explained.Percentage composition in following embodiment is if no special instructions
It is weight/mass percentage composition.
Embodiment 1
By 2mmolAlCl3·6H2O and 36mmol CO (NH2)2Join in the middle of the deionized water of 50mL, then
Constantly agitating solution, until becoming homogeneous phase solution.By the time, after solution becomes clarification, at once solution is transferred to 100mL
In the middle of the reactor of inner liner polytetrafluoroethylene, then reactor is reacted at 140 DEG C 36h.Arrive between when reacted and set
Time time, take out reactor, naturally cool to room temperature.By filtering, wash the reacted product of collection after cooling.
The last product will collected again dry 24h, i.e. obtained solid base catalyst NH at 100 DEG C4Al(OH)2CO3。
This product carries out XRD analysis, and XRD spectrum is as it is shown in figure 1, it can be seen that at 2 θ=10～80 °
There is the strongest diffraction maximum, all of diffraction maximum (JCPDS Card consistent with the standard card figure of aluminum carbonate basic ammonium
042-0250), the composition that this product is described is NH4Al(OH)2CO3。
First by the solid base catalyst NH of 0.1g glucose and 0.3g4Al(OH)2CO3Join 1g1-butyl-3-methyl
In the mixed solution of imidazoles villaumite and 1g dimethyl sulfoxide (DMSO), then said mixture is quickly transferred in 120 DEG C of oil baths
Stirring reaction 4h, obtains reacted mixture energetically.Quench obtained liquid adds deionized water,
Separate 10min with centrifuge with the speed of 10000rpm again, collect upper strata hydrolyzate, both obtained 5 hydroxymethyl furfural, and produced
Thing ultraviolet specrophotometer is analyzed, and the productivity of 5 hydroxymethyl furfural is 42.17wt%.
Embodiment 2
By 2mmolAlCl3·6H2O and 54mmolCO (NH2)2Join in the middle of the deionized water of 50mL, the most not
Disconnected ground agitating solution, until becoming homogeneous phase solution.By the time, after solution becomes clarification, at once solution is transferred to 100mL
In the middle of the reactor of inner liner polytetrafluoroethylene, then reactor is reacted at 140 DEG C 36h.Arrive between when reacted and set
Time time, take out reactor, naturally cool to room temperature.By filtering, wash the reacted product of collection after cooling.
The last product will collected again dry 24h, i.e. obtained solid base catalyst NH at 100 DEG C4Al(OH)2CO3。
First by the solid base catalyst NH of 0.1g glucose and 0.3g4Al(OH)2CO3Join 1g1-butyl-3-methyl miaow
In the mixed solution of azoles villaumite and 1g dimethyl sulfoxide (DMSO).Then said mixture is quickly transferred in 120 DEG C of oil baths energetically
Stirring reaction 4h, obtains reacted mixture.By in obtained liquid add deionized water quench, then with from
Scheming separates 10min with the speed of 10000rpm, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and product is purple
Outer spectrophotometer is analyzed, and the productivity of 5 hydroxymethyl furfural is 39.31wt%.
Embodiment 3
By 2mmolAlCl3·6H2O and 72mmolCO (NH2)2Join in the middle of the deionized water of 50mL, the most not
Disconnected ground agitating solution, until becoming homogeneous phase solution.By the time, after solution becomes clarification, at once solution is transferred to 100mL
In the middle of the reactor of inner liner polytetrafluoroethylene, then reactor is reacted at 140 DEG C 36h.Arrive between when reacted and set
Time time, take out reactor, naturally cool to room temperature.By filtering, wash the reacted product of collection after cooling.
The last product will collected again dry 24h, i.e. obtained solid base catalyst NH at 100 DEG C4Al(OH)2CO3。
First by the solid base catalyst NH of 0.1g glucose and 0.3g4Al(OH)2CO3Join 1g1-butyl-3-methyl miaow
In the mixed solution of azoles villaumite and 1g dimethyl sulfoxide (DMSO).Then said mixture is quickly transferred in 120 DEG C of oil baths energetically
Stirring reaction 4h, obtains reacted mixture.By in obtained liquid add deionized water quench, then with from
Scheming separates 10min, upper collection upper strata hydrolyzate with the speed of 10000rpm, has both obtained 5 hydroxymethyl furfural, and product is used
Ultraviolet specrophotometer is analyzed, and the productivity of 5 hydroxymethyl furfural is 33.51wt%.
Embodiment 4
By 2mmol aluminium isopropoxide C9H21AlO3With 36mmol NH4HCO3The deionized water joining 50mL work as
In, the most constantly agitating solution, until becoming homogeneous phase solution.By the time, after solution becomes clarification, at once solution is turned
Move on in the middle of the reactor of 100mL inner liner polytetrafluoroethylene, then reactor is reacted at 140 DEG C 36h.Work as reaction
When time arrives the time set, take out reactor, naturally cool to room temperature.By filtering, wash collection instead after cooling
Product after should.The last product will collected again dry 24h, i.e. obtained solid base catalyst at 100 DEG C
NH4Al(OH)2CO3。
First by the solid base catalyst NH of 0.1g glucose and 0.3g4Al(OH)2CO3Join 1g1-butyl-3-methyl
In the mixed solution of imidazoles villaumite and 1g dimethyl sulfoxide (DMSO).Then said mixture is quickly transferred in 120 DEG C of oil baths
Stirring reaction 4h, obtains reacted mixture energetically.Quench obtained liquid adds deionized water,
Separate 10min, upper collection upper strata hydrolyzate with centrifuge with the speed of 10000rpm again, both obtain 5 hydroxymethyl furfural,
Product ultraviolet specrophotometer is analyzed, and the productivity of 5 hydroxymethyl furfural is 35.23wt%.
Embodiment 5
By 2mmol aluminium isopropoxide C9H21AlO3With 36mmol (NH4)2CO3The deionized water joining 50mL
In the middle of, the most constantly agitating solution, until becoming homogeneous phase solution.By the time after solution becomes clarification, at once solution
Transfer in the middle of the reactor of 100mL inner liner polytetrafluoroethylene, then reactor is reacted at 140 DEG C 36h.When instead
When arriving the time of setting between Ying Shi, take out reactor, naturally cool to room temperature.By filtering, washing collection after cooling
Reacted product.The last product will collected again dry 24h, i.e. obtained solid base catalyst at 100 DEG C
NH4Al(OH)2CO3。
First by the solid base catalyst NH of 0.1g glucose and 0.3g4Al(OH)2CO3Join 1g1-butyl-3-methyl
In the mixed solution of imidazoles villaumite and 1g dimethyl sulfoxide (DMSO).Then said mixture is quickly transferred in 120 DEG C of oil baths
Stirring reaction 4h, obtains reacted mixture energetically.Quench obtained liquid adds deionized water,
Separate 10min, upper collection upper strata hydrolyzate with centrifuge with the speed of 10000rpm again, both obtain 5 hydroxymethyl furfural,
Product ultraviolet specrophotometer is analyzed, and the productivity of 5 hydroxymethyl furfural is 32.19wt%.
Embodiment 6
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1, simply by aluminium source AlCl3·6H2O becomes
For C9H21AlO3.It is applied to glucose conversion with the catalyst that will prepare prepare in 5 hydroxymethyl furfural test.By 0.1
The solid base catalyst NH of g glucose and 0.3g4Al(OH)2CO3Join 1g1-butyl-3-methylimidazole villaumite and 1
In the mixed solution of g dimethyl sulfoxide (DMSO).Then it is quickly transferred to said mixture reaction is stirred in 120 DEG C of oil baths energetically
4h, obtains reacted mixture.By in obtained liquid add deionized water quench, then with centrifuge with
The speed of 10000rpm separates 10min, upper collection upper strata hydrolyzate, has both obtained 5 hydroxymethyl furfural, and product ultraviolet is divided
Light photometer is analyzed, and the productivity of 5 hydroxymethyl furfural is 37.25wt%.From experimental result it can be seen that use
C9H21AlO3The most considerable as aluminium source productivity, and C9H21AlO3It is octahedra with Al atom for hexa-coordinate
Structure, potentially contribute to formed catalyst n H4Al(OH)2CO3。
Embodiment 7
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By consolidating of 0.1g glucose and 0.1g
Body base catalyst NH4Al(OH)2CO3The mixing joining 1g1-butyl-3-methylimidazole villaumite and 1g dimethyl sulfoxide (DMSO) is molten
In liquid.Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixing
Thing.Quench obtained liquid adds deionized water, then separate with the speed of 10000rpm with centrifuge
10min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and product ultraviolet specrophotometer is analyzed, 5-hydroxyl
The productivity of methyl furfural is 29.04wt%.
Embodiment 8
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By consolidating of 0.1g glucose and 0.2g
Body base catalyst NH4Al(OH)2CO3The mixing joining 1g1-butyl-3-methylimidazole villaumite and 1g dimethyl sulfoxide (DMSO) is molten
In liquid.Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixing
Thing.Quench obtained liquid adds deionized water, then separate with the speed of 10000rpm with centrifuge
10min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and product ultraviolet specrophotometer is analyzed, 5-hydroxyl
The productivity of methyl furfural is 39.60wt%.
Embodiment 9
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By consolidating of 0.1g glucose and 0.4g
Body base catalyst NH4Al(OH)2CO3The mixing joining 1g1-butyl-3-methylimidazole villaumite and 1g dimethyl sulfoxide (DMSO) is molten
In liquid.Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixing
Thing.Quench obtained liquid adds deionized water, then separate with the speed of 10000rpm with centrifuge
10min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and product ultraviolet specrophotometer is analyzed, 5-hydroxyl
The productivity of methyl furfural is 35.45wt%.
Embodiment 10
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By consolidating of 0.1g glucose and 0.5g
Body base catalyst NH4Al(OH)2CO3The mixing joining 1g1-butyl-3-methylimidazole villaumite and 1g dimethyl sulfoxide (DMSO) is molten
In liquid.Then said mixture is quickly transferred in 120 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixing
Thing.Quench obtained liquid adds deionized water, then separate with the speed of 10000rpm with centrifuge
10min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and product ultraviolet specrophotometer is analyzed, 5-hydroxyl
The productivity of methyl furfural is 28.81wt%.
Embodiment 11
Solid base catalyst NH4Al(OH)2CO3Preparation method with embodiment 1.By consolidating of 0.1g glucose and 0.3g
Body base catalyst NH4Al(OH)2CO3The mixing joining 1g1-butyl-3-methylimidazole villaumite and 1g dimethyl sulfoxide (DMSO) is molten
In liquid.Then said mixture is quickly transferred in 140 DEG C of oil baths stirring reaction 4h energetically, obtains reacted mixing
Thing.Quench obtained liquid adds deionized water, then separate with the speed of 10000rpm with centrifuge
10min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and product ultraviolet specrophotometer is analyzed, 5-hydroxyl
The productivity of methyl furfural is 25.66wt%.
Embodiment 12
The solid base catalyst NH of embodiment 1 preparation4Al(OH)2CO3Recycling.
Solid base catalyst NH4Al(OH)2CO3NH4 +Easily running off, therefore catalyst is separating, is washing after drying
Need again could recycle through ammonia treatment.Concretely comprise the following steps: the solid base catalyst after separating
NH4Al(OH)2CO3It is immersed in 25wt% concentrated ammonia liquor, stirs 24h energetically.Then refilter, wash 10 times, left
After at 100 DEG C be dried 24h.Finally under the conditions of same as in Example 1, it is catalyzed glucose with this catalyst circulated to turn
Changing, the productivity obtaining 5 hydroxymethyl furfural is 44.22wt%.The circulation operation of same catalyst, 5 hydroxymethyl furfural
Yield results as shown in table 1.As it can be seen from table 1 this catalyst all remains, in 5 circulations, the 5-that comparison is high
The productivity of hydroxymethylfurfural.
The NH of table 1 embodiment 1 preparation4Al(OH)2CO3The access times impact on 5 hydroxymethyl furfural productivity
| Catalyst access times | 5 hydroxymethyl furfural productivity (wt%) |
| 1 | 42.17 |
| 2 | 44.22 |
| 3 | 42.05 |
| 4 | 41.23 |
| 5 | 40.37 |
Above description is for implementing some optimal modes of the present invention and other embodiments, the simply technology to the present invention
Design play description example effect, can not limit the scope of the invention with this, those skilled in the art without departing from
In the spirit and scope of technical solution of the present invention, modify and equivalent, all should fall protection scope of the present invention it
In.
Claims (9)
1. a solid base catalyst NH4Al(OH)2CO3, it is characterised in that: described solid base catalyst
NH4Al(OH)2CO3Be with inorganic salt containing aluminium and/or aluminium isopropoxide be aluminium source, urea CO (NH2)2For precipitating reagent
Directly synthesized by hydrothermal solution without calcining and activating.
Solid base catalyst NH the most according to claim 14Al(OH)2CO3, it is characterised in that: institute
State inorganic salt containing aluminium selected from AlCl3、Al(NO3)3、Al2(SO4)3、AlCl3·6H2O、Al(NO3)3·9H2O、
Al2(SO4)3·16H2One or more in O.
Solid base catalyst NH the most according to claim 1 and 24Al(OH)2CO3Preparation method,
It is characterized in that: described preparation method comprises the following steps:
(1) using as the inorganic salt containing aluminium in aluminium source and/or aluminium isopropoxide and CO (NH2)2Join deionized water
In, the most constantly agitating solution, until becoming homogeneous phase solution；
(2), after the homogeneous phase solution obtained until step (1) becomes clarification, at once solution is transferred to 100～200mL
Reaction in the middle of the reactor of inner liner polytetrafluoroethylene, then reactor is reacted at 100～300 DEG C 5～60h, when
When reaction time arrives the time set, take out reactor, naturally cool to room temperature；
(3) by filtering, wash the reacted product of collection after cooling, finally it is dried at 60～150 DEG C
3～48h, i.e. obtain solid base catalyst NH4Al(OH)2CO3。
Solid base catalyst NH the most according to claim 34Al(OH)2CO3Preparation method, it is special
Levy and be: aluminium source and CO (NH in described step (1)2)2The ratio of amount of material be 1-10:1-200.
5. a solid base catalyst NH according to claim 14Al(OH)2CO3Catalyzed conversion grape
The method of sugar, it is characterised in that: comprise the following steps:
(1) first by glucose and described solid base catalyst NH4Al(OH)2CO3Join in solvent, obtain
Mixture A；
(2) then it is quickly transferred in oil bath stir reaction energetically by the mixture A that step (1) obtains,
Obtain reacted mixture B；
(3) the mixture B that step (2) obtained adds deionized water and quenches, then with centrifuge with
The speed of 5000～20000rpm separates 3～15min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and produced
Thing ultraviolet specrophotometer is analyzed.
Solid base catalyst NH the most according to claim 54Al(OH)2CO3Catalyzed conversion glucose
Method, it is characterised in that: in described step (1), solvent is 1-butyl-3-methylimidazole villaumite, dimethyl Asia
The one or both mixing of sulfone.
Solid base catalyst NH the most according to claim 54Al(OH)2CO3Catalyzed conversion glucose
Method, it is characterised in that: in described step (1), solid base catalyst is 3:1 with the mass ratio of glucose.
Solid base catalyst NH the most according to claim 54Al(OH)2CO3Catalyzed conversion glucose
Method, it is characterised in that: in described step (2), the temperature of oil bath is 60～180 DEG C, described stirring reaction
Time be 2～12h.
9. according to the solid base catalyst NH described in any one of claim 5-84Al(OH)2CO3Catalyzed conversion Portugal
The method of grape sugar, it is characterised in that:
(1) first by 0.01～1g glucose and the solid base catalyst NH of 0.01～5g4Al(OH)2CO3Add
In the solvent of 0～10g1-butyl-3-methylimidazole villaumite and 0～10g dimethyl sulfoxide (DMSO), obtain mixture A,
Wherein 1-butyl-3-methylimidazole villaumite is 0 time different with dimethyl sulfoxide (DMSO)；
(2) then it is quickly transferred to the mixture A that step (1) obtains in 60～180 DEG C of oil baths stir energetically
Mix reaction 2～12h, obtain reacted mixture B；
(3) in the liquid that step (2) is obtained add deionized water quench, then with centrifuge with
The speed of 5000～20000rpm separates 3～15min, collects upper strata hydrolyzate, had both obtained 5 hydroxymethyl furfural, and produced
Thing ultraviolet specrophotometer is analyzed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610237172.XA CN105749946B (en) | 2016-04-15 | 2016-04-15 | A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201610237172.XA CN105749946B (en) | 2016-04-15 | 2016-04-15 | A kind of solid base catalyst NH4Al(OH)2CO3, preparation method and its catalyzed conversion glucose method |
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| CN108610311A (en) * | 2018-05-30 | 2018-10-02 | 盐城工学院 | A kind of method that the low-temperature catalyzed glucose of boehmite prepares 5 hydroxymethyl furfural |
| CN113845552A (en) * | 2020-11-06 | 2021-12-28 | 南开大学 | Method for catalyzing isomerization of glucose into fructose by using solid base |
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| CN108610311A (en) * | 2018-05-30 | 2018-10-02 | 盐城工学院 | A kind of method that the low-temperature catalyzed glucose of boehmite prepares 5 hydroxymethyl furfural |
| CN108610311B (en) * | 2018-05-30 | 2021-12-10 | 盐城工学院 | Method for preparing 5-hydroxymethylfurfural by using boehmite to catalyze glucose at low temperature |
| CN113845552A (en) * | 2020-11-06 | 2021-12-28 | 南开大学 | Method for catalyzing isomerization of glucose into fructose by using solid base |
| CN113845552B (en) * | 2020-11-06 | 2024-01-05 | 南开大学 | Method for catalyzing glucose to isomerise into fructose by using solid base |
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